CN107557004A - A kind of method for preparing stable perovskite quantum dot - Google Patents
A kind of method for preparing stable perovskite quantum dot Download PDFInfo
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- CN107557004A CN107557004A CN201710964871.9A CN201710964871A CN107557004A CN 107557004 A CN107557004 A CN 107557004A CN 201710964871 A CN201710964871 A CN 201710964871A CN 107557004 A CN107557004 A CN 107557004A
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- quantum dot
- silicon oxide
- mesoporous silicon
- lead halide
- presoma
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Abstract
A kind of method for preparing stable perovskite quantum dot, utilize the principle of physical absorption, the lead halide presoma for preparing perovskite quantum dot is embedded into the aperture of mesoporous silicon oxide, then the mesoporous silicon oxide of embedded lead halide presoma is immersed in oleic acid caesium presoma, after stirring, sonic oscillation, mesoporous silicon oxide stable in the air/perovskite quantum dot is obtained.The present invention proposes a kind of method for preparing stable perovskite quantum dot, and the perovskite quantum dot for wrapping up the mesoporous silicon oxide of acquisition keeps long-term stability and has high quantum yield in atmosphere.
Description
Technical field
The present invention relates to a kind of method for preparing stable perovskite quantum dot, luminescent material technical field is particularly belonged to.
Background technology
In recent years, perovskite quantum dot turns into the newcomer in " quantum dot family ", has that emission wavelength is narrow, luminescence generated by light
Outstanding advantages of efficiency high, Color tunable, excitation are high, quantum yield is high, band gap is adjustable, it is a kind of new with growing potential
Type quanta point material.And because its excellent Inherent Optical Properties opens the potential application in fields such as display, illumination and laser.
At present, perovskite quantum dot is mainly applied in light emitting diode, solar-electricity in the form of two kinds of solution and fluorescent material
In the photoelectric devices such as pond, but the perovskite quantum dot stability that at present prepared by technology is poor, in atmosphere easily by materials such as water, oxygen
Burn into decomposes.Its stability difference governs its development always.Therefore, how to ensure that perovskite quantum dot is kept in atmosphere
Long-term stabilization, turns into urgent need to solve the problem.In recent years, for the research for the stability for how improving perovskite quantum dot
Compare more, general idea is that perovskite quantum dot is wrapped in inside a certain stable material, such as in titanium dioxide, silica
Deng, or change the surface ligand of perovskite quantum dot, such as use hexane and ethyl acetate mixed solvent.Titanium dioxide is used above-mentioned
In the research of silicon parcel perovskite quantum dot, most of research is to hydrolyze to form dioxy using APTES
SiClx matrix.And the present invention then proposes a kind of to synthesize the method for perovskite quantum dot in the aperture of mesoporous silicon oxide.Phase
Method than obtaining silica matrix with other Hydrolyze methods, the present invention is directly to use meso-porous titanium dioxide silicon matrix, is prepared
Journey is simple.And final perovskite quantum dot is embedded in the aperture of mesoporous silicon oxide, can not only protect quantum dot from
The erosion of water, oxygen, the problem of improving its stability difference, and can also allow the influence from anion exchange reaction, avoid simultaneously
Reunion between quantum dot, improves quantum yield.
The content of the invention
In order to solve the problems, such as perovskite quantum dot stability difference, the present invention provides one kind and prepares stable perovskite quantum dot
Method, the perovskite quantum dot for the mesoporous silicon oxide parcel being prepared based on this method can keep long-term in atmosphere
Stability simultaneously has high quantum yield.
To achieve the above object, it is of the invention:Using the principle of physical absorption, by before the lead halide for preparing perovskite quantum dot
Drive body to be embedded into the aperture of mesoporous silicon oxide, the mesoporous silicon oxide of embedded lead halide presoma is then immersed in oleic acid
In caesium presoma, after stirring, sonic oscillation, mesoporous silicon oxide stable in the air/perovskite quantum dot is obtained.
Comprise the following steps that：
Step 1：The preparation of oleic acid caesium presoma
Cesium carbonate, octadecylene and oleic acid are added in flask, vacuum outgas to -30bar, and are heated to 50-100 DEG C, kept
After 20-40 minutes, it is filled with nitrogen and is heated to 120-140 DEG C, be incubated 2-10 minutes, until solution is clarified, prepares oleic acid caesium
Presoma.
Step 2：The preparation of lead halide presoma
By lead halide（PbX2）, octadecylene (1-ODE), oleic acid (OA) and oleyl amine (OAM) be added in flask, heat under vacuo
To 50-100 DEG C, after being kept for 20-40 minutes, nitrogen protection is filled with, and is heated to 170-190 DEG C, until solution becomes clarification, is prepared
Go out lead halide presoma.
Step 3：The preparation of the mesoporous silicon oxide of embedded lead halide
Take lead halide presoma to be placed in flask, add mesoporous silicon oxide, 70-190 DEG C is stirred and heated under vacuum, ultrasound
After vibrating 1-120 minutes, by centrifugal treating, remove supernatant, obtain being embedded in the mesoporous silicon oxide of lead halide.
Step 4：The preparation of stable perovskite quantum dot
Take oleic acid caesium presoma to be placed in flask, add the mesoporous silicon oxide of described insertion lead halide, stir and ultrasound is shaken
After swinging 1-120 minutes, room temperature is cooled to, by centrifugal treating, removes supernatant, the calcium titanium of obtained mesoporous silicon oxide parcel
Ore deposit quantum dot fluorescence powder through n-hexane and toluene washing, vacuum drying, obtains stablizing perovskite quantum dot respectively.
Beneficial effects of the present invention：
1st, the present invention, which proposes, is embedded into perovskite quantum dot in mesoporous silicon oxide, wraps up the mesoporous silicon oxide of acquisition
Perovskite quantum dot can keep long-term stability in atmosphere.
2nd, the present invention, which proposes, is first embedded into lead halide in mesoporous silicon oxide, then is immersed in oleic acid caesium presoma anti-
Should, prepare stable mesoporous silicon oxide/perovskite quantum dot.
3rd, the perovskite quantum dot for the mesoporous silicon oxide parcel that prepared by the present invention has high fluorescence quantum yield.
Embodiment
It is described in further detail by the following examples, but the present embodiment is not intended to limit the invention, every use
The similar structure of the present invention and its similar change, all should be included in protection scope of the present invention.
Chemical material：Carbonic acid is gorgeous（CsCO3, 99.9%）, oleic acid（OA, 90%）, octadecylene（1-ODE, 90%）, lead bromide
（PbBr2, 99.0%）, lead iodide（PbI2, 99.0%）, lead chloride（PbCl2）, n-octyl phosphine（TOP, 90%）N-hexane（99.5%）
And toluene（99.5%）, oleyl amine（OAM, 90.0%）, mesoporous silicon oxide.
Embodiment 1
1）The preparation of oleic acid caesium presoma：By 0.4g cesium carbonates CsCO3, 5ml octadecylene 1-ODE and 0.4ml oleic acid OA, be added to
In 25ml three neck round bottom, deaerated under vacuum 10 minutes, and 70 DEG C are heated to, 70 DEG C of holding is constant, and vacuum outgas 30 divides
Zhong Hou, nitrogen protection is filled with, and is heated to 130 DEG C, be incubated 10 minutes, until solution is clarified.
2）The preparation of lead halide presoma：By 0.069g PbX3（Blue quantum dot：0.034g PbBr2, 0.026g
PbCl2, 1ml TOP；Green quantum dot：0.069g PbBr2；Red quantum dot：0.065g PbBr2, 0.0172g PbBr2）,
5ml octadecylenes 1-ODE, 0.5ml oleic acid OA and 0.5ml oleyl amine OAM, is added in 25ml three neck round bottom, is taken off under vacuum
Gas 10 minutes, and be heated to 70 DEG C, keep 70 DEG C it is constant, after vacuum outgas 30 minutes, be filled with nitrogen protection, and be heated to 180
DEG C, until solution becomes clarification.
3）The preparation of the mesoporous silicon oxide of embedded lead halide：5ml lead halide presomas are taken to be placed in 25ml three neck round bottoms
In flask, mesoporous silicon oxide is added, is stirred and heated to 130 DEG C under vacuum, sonic oscillation is after 60 minutes, by 4000rpm
Centrifugation 5 minutes, removes supernatant, obtains being embedded in the mesoporous silicon oxide of lead halide.
4）Mesoporous silicon oxide wraps up the preparation of perovskite quantum dot：5ml oleic acid caesium presomas are taken to be placed in 25ml three necks
In round-bottomed flask, the mesoporous silicon oxide of described insertion lead halide is added, is stirred and heated to 80 DEG C, sonic oscillation 60 minutes
Afterwards, room temperature is cooled to, is centrifuged 5 minutes in 4000rpm, removes supernatant, obtains the perovskite quantum of mesoporous silicon oxide parcel
Dot fluorescent powder, and cleaned respectively with n-hexane and toluene, 100 DEG C are dried in vacuo 1 hour in vacuum drying chamber.
Embodiment 2
1）The preparation of oleic acid caesium presoma：By 0.4g cesium carbonates CsCO3, 5ml octadecylene 1-ODE and 0.4ml oleic acid OA, be added to
In 25ml three neck round bottom, deaerated under vacuum 10 minutes, and 100 DEG C are heated to, keep 100 DEG C of constant, vacuum outgas 20
After minute, nitrogen protection is filled with, and is heated to 130 DEG C, is incubated 10 minutes, until solution is clarified.
2）The preparation of lead halide presoma：By 0.069g PbX3（Blue quantum dot：0.034g PbBr2, 0.026g
PbCl2, 1ml TOP；Green quantum dot：0.069g PbBr2；Red quantum dot：0.065g PbBr2, 0.0172g PbBr2）,
5ml octadecylenes 1-ODE, 0.5ml oleic acid OA and 0.5ml oleyl amine OAM, is added in 25ml three neck round bottom, is taken off under vacuum
Gas 10 minutes, and be heated to 70 DEG C, keep 70 DEG C it is constant, after vacuum outgas 30 minutes, be filled with nitrogen protection, and be heated to 180
DEG C, until solution becomes clarification.
3）The preparation of the mesoporous silicon oxide of embedded lead halide：5ml lead halide presomas are taken to be placed in 25ml three neck round bottoms
In flask, add mesoporous silicon oxide, be stirred and heated to 70 DEG C under vacuum, sonic oscillation is after 60 minutes, by 4000rpm from
The heart 5 minutes, removes supernatant, obtains being embedded in the mesoporous silicon oxide of lead halide.
4）Mesoporous silicon oxide wraps up the preparation of perovskite quantum dot：5ml oleic acid caesium presomas are taken to be placed in 25ml three necks
In round-bottomed flask, the mesoporous silicon oxide of described insertion lead halide is added, is stirred and heated to 80 DEG C, sonic oscillation 60 minutes
Afterwards, room temperature is cooled to, is centrifuged 5 minutes in 4000rpm, removes supernatant, obtains the perovskite quantum of mesoporous silicon oxide parcel
Dot fluorescent powder, and cleaned respectively with n-hexane and toluene, 100 DEG C are dried in vacuo 1 hour in vacuum drying chamber.
Embodiment 3
1）The preparation of oleic acid caesium presoma：By 0.4g cesium carbonates CsCO3, 5ml octadecylene 1-ODE and 0.4ml oleic acid OA, be added to
In 25ml three neck round bottom, deaerated under vacuum 10 minutes, and 50 DEG C are heated to, 50 DEG C of holding is constant, and vacuum outgas 40 divides
Zhong Hou, nitrogen protection is filled with, and is heated to 130 DEG C, be incubated 10 minutes, until solution is clarified.
2）The preparation of lead halide presoma：By 0.069g PbX3（Blue quantum dot：0.034g PbBr2, 0.026g
PbCl2, 1ml TOP；Green quantum dot：0.069g PbBr2；Red quantum dot：0.065g PbBr2, 0.0172g PbBr2）,
5ml octadecylenes 1-ODE, 0.5ml oleic acid OA and 0.5ml oleyl amine OAM, is added in 25ml three neck round bottom, is taken off under vacuum
Gas 10 minutes, and be heated to 70 DEG C, keep 70 DEG C it is constant, after vacuum outgas 30 minutes, be filled with nitrogen protection, and be heated to 180
DEG C, until solution becomes clarification.
3）The preparation of the mesoporous silicon oxide of embedded lead halide：5ml lead halide presomas are taken to be placed in 25ml three neck round bottoms
In flask, add mesoporous silicon oxide, be stirred and heated to 70 DEG C under vacuum, sonic oscillation is after 60 minutes, by 4000rpm from
The heart 5 minutes, removes supernatant, obtains being embedded in the mesoporous silicon oxide of lead halide.
4）Mesoporous silicon oxide wraps up the preparation of perovskite quantum dot：5ml oleic acid caesium presomas are taken to be placed in 25ml three necks
In round-bottomed flask, the mesoporous silicon oxide of described insertion lead halide is added, is stirred and heated to 80 DEG C, sonic oscillation 120 divides
Zhong Hou, room temperature is cooled to, is centrifuged 5 minutes in 4000rpm, remove supernatant, obtain the perovskite amount of mesoporous silicon oxide parcel
Sub- dot fluorescent powder, and cleaned respectively with n-hexane and toluene, 100 DEG C are dried in vacuo 1 hour in vacuum drying chamber.
Claims (1)
- A kind of 1. method for preparing stable perovskite quantum dot, it is characterised in that：Described method utilizes the principle of physical absorption, The lead halide presoma for preparing perovskite quantum dot is embedded into the aperture of mesoporous silicon oxide, then by before embedded lead halide The mesoporous silicon oxide for driving body is immersed in oleic acid caesium presoma, after stirring, sonic oscillation, is obtained stable in the air Mesoporous silicon oxide/perovskite quantum dot；Comprise the following steps that：Step 1：The preparation of oleic acid caesium presomaCesium carbonate, octadecylene and oleic acid are added in flask, vacuum outgas to -30bar, and are heated to 50-100 DEG C, kept After 20-40 minutes, it is filled with nitrogen and is heated to 120-140 DEG C, be incubated 2-10 minutes, until solution is clarified, prepares oleic acid caesium Presoma；Step 2：The preparation of lead halide presomaLead halide, octadecylene, oleic acid and oleyl amine are added in flask, are heated to 50-100 DEG C under vacuo, is kept for 20-40 points Zhong Hou, nitrogen protection is filled with, and is heated to 170-190 DEG C, until solution becomes clarification, prepare lead halide presoma；Step 3：The preparation of the mesoporous silicon oxide of embedded lead halideTake lead halide presoma to be placed in flask, add mesoporous silicon oxide, 70-190 DEG C is stirred and heated under vacuum, ultrasound After vibrating 1-120 minutes, by centrifugal treating, remove supernatant, obtain being embedded in the mesoporous silicon oxide of lead halide；Step 4：The preparation of stable perovskite quantum dotTake oleic acid caesium presoma to be placed in flask, add the mesoporous silicon oxide of described insertion lead halide, stir and ultrasound is shaken After swinging 1-120 minutes, room temperature is cooled to, by centrifugal treating, removes supernatant, the calcium titanium of obtained mesoporous silicon oxide parcel Ore deposit quantum dot fluorescence powder through n-hexane and toluene washing, vacuum drying, obtains stablizing perovskite quantum dot respectively.
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Cited By (13)
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|---|---|---|---|---|
| CN108767125A (en) * | 2018-05-21 | 2018-11-06 | 电子科技大学 | A kind of QD-3D-QD luminescent layers perovskite light emitting diode and preparation method thereof |
| CN108841387A (en) * | 2018-07-18 | 2018-11-20 | 深圳扑浪创新科技有限公司 | A kind of quantum nanoparticles crystalline substance compound and preparation method thereof |
| CN109021283A (en) * | 2018-04-19 | 2018-12-18 | 华南师范大学 | For detecting the CsPbBr of flolimat3Perovskite quantum dot-molecular engram fluorescent optical sensor and preparation method thereof |
| CN109586155A (en) * | 2018-12-07 | 2019-04-05 | 东南大学 | Based on mesoporous SiO2The accidental laser of spherical shell combination of inner and outside quantum dot film |
| CN109802044A (en) * | 2019-01-07 | 2019-05-24 | 东华大学 | A kind of method of room temperature preparation high quality perovskite thin film |
| CN110205110A (en) * | 2019-05-05 | 2019-09-06 | 厦门大学 | Duct confinement-shell isolated duplicate protection perovskite nanoparticle preparation method |
| CN111103274A (en) * | 2019-12-23 | 2020-05-05 | 厦门大学 | Method for rapidly detecting lead ions in sample liquid |
| CN111349436A (en) * | 2018-12-24 | 2020-06-30 | Tcl集团股份有限公司 | Preparation method of quantum dots |
| CN111454713A (en) * | 2020-04-10 | 2020-07-28 | 南通创亿达新材料股份有限公司 | Perovskite quantum dot powder, preparation method thereof and perovskite quantum dot functional material |
| CN111518558A (en) * | 2019-12-11 | 2020-08-11 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| WO2021046956A1 (en) * | 2019-09-09 | 2021-03-18 | 武汉华星光电半导体显示技术有限公司 | Modified perovskite quantum dot material, preparation method therefor, and display device |
| CN114058367A (en) * | 2021-12-17 | 2022-02-18 | 兰州大学 | Perovskite quantum dot and mesoporous silica composite luminescent material and preparation thereof |
| US11332661B2 (en) | 2019-09-09 | 2022-05-17 | Wuhan China Star Optoelectronics Semiconductor Display Technology Co., Ltd. | Modified perovskite quantum dot material, fabricating method thereof, and display device |
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| CN109021283A (en) * | 2018-04-19 | 2018-12-18 | 华南师范大学 | For detecting the CsPbBr of flolimat3Perovskite quantum dot-molecular engram fluorescent optical sensor and preparation method thereof |
| CN109021283B (en) * | 2018-04-19 | 2021-01-26 | 华南师范大学 | CsPbBr for detecting omethoate3Perovskite quantum dot-molecularly imprinted fluorescent sensor and preparation method thereof |
| CN108767125A (en) * | 2018-05-21 | 2018-11-06 | 电子科技大学 | A kind of QD-3D-QD luminescent layers perovskite light emitting diode and preparation method thereof |
| CN108767125B (en) * | 2018-05-21 | 2019-07-05 | 电子科技大学 | A kind of QD-3D-QD luminescent layer perovskite light emitting diode and preparation method thereof |
| CN108841387A (en) * | 2018-07-18 | 2018-11-20 | 深圳扑浪创新科技有限公司 | A kind of quantum nanoparticles crystalline substance compound and preparation method thereof |
| CN109586155A (en) * | 2018-12-07 | 2019-04-05 | 东南大学 | Based on mesoporous SiO2The accidental laser of spherical shell combination of inner and outside quantum dot film |
| CN111349436A (en) * | 2018-12-24 | 2020-06-30 | Tcl集团股份有限公司 | Preparation method of quantum dots |
| CN109802044A (en) * | 2019-01-07 | 2019-05-24 | 东华大学 | A kind of method of room temperature preparation high quality perovskite thin film |
| CN110205110A (en) * | 2019-05-05 | 2019-09-06 | 厦门大学 | Duct confinement-shell isolated duplicate protection perovskite nanoparticle preparation method |
| CN110205110B (en) * | 2019-05-05 | 2020-07-10 | 厦门大学 | Preparation method of pore confinement-shell isolation double-protection perovskite nano particles |
| WO2021046956A1 (en) * | 2019-09-09 | 2021-03-18 | 武汉华星光电半导体显示技术有限公司 | Modified perovskite quantum dot material, preparation method therefor, and display device |
| US11332661B2 (en) | 2019-09-09 | 2022-05-17 | Wuhan China Star Optoelectronics Semiconductor Display Technology Co., Ltd. | Modified perovskite quantum dot material, fabricating method thereof, and display device |
| CN111518558A (en) * | 2019-12-11 | 2020-08-11 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| CN111518558B (en) * | 2019-12-11 | 2021-10-26 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| CN111103274A (en) * | 2019-12-23 | 2020-05-05 | 厦门大学 | Method for rapidly detecting lead ions in sample liquid |
| CN111103274B (en) * | 2019-12-23 | 2021-04-20 | 厦门大学 | Method for rapidly detecting lead ions in sample liquid |
| CN111454713A (en) * | 2020-04-10 | 2020-07-28 | 南通创亿达新材料股份有限公司 | Perovskite quantum dot powder, preparation method thereof and perovskite quantum dot functional material |
| CN114058367A (en) * | 2021-12-17 | 2022-02-18 | 兰州大学 | Perovskite quantum dot and mesoporous silica composite luminescent material and preparation thereof |
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